Search Results (23)

Water pollution by antibiotics and heavy metals threatens the ecological environment and human health globally, yet there is no rapid method to detect multiple antibiotics and metal ions simultaneously. A simple, fast, and ultra-sensitive colorimetric chemosensor for the simultaneous detection of moxifloxacin (MOX), ciprofloxacin (CIP), and Cr(III) based on the aggregation of ammonium thioglycolate (ATG)-functionalized gold nanoparticles (ATG-AuNPs) was developed. Following the addition of MOX, CIP, and Cr(III), a color change in the solution was observed from wine-red to blue-grey. The UV–Vis signal of the ATG-AuNPs system blended with MOX, CIP, and Cr(III) in the range of 0~200 µM, 0~100 µM, and 0~5 µM was assessed and measured with detection limits (LODs) of 1.57 µM, 1.30 µM, and 57.1 nM calculated by 3σ/S, respectively. Therefore, this system has the potential to act as an effective colorimetric chemosensor for simultaneously detecting MOX, CIP, and Cr(III) in complex environmental systems. Full article

Traditional detection methods such as atomic absorption spectroscopy offer high sensitivity and accuracy for heavy metal ion detection; however, they are often limited to laboratory environments due to bulky equipment and complex procedures. To meet the demand for rapid on-site detection, this study employs electrochemical analysis and utilizes Micro-Electro-Mechanical Systems (MEMS) technology to fabricate a microelectrode sensor chip for the electrochemical detection of heavy metal ions, Hg(II) and As(III). Nano-gold particles were electrodeposited on the sensing area of the working electrode of this chip using a constant-potential deposition method. Uniform distribution of the nanoparticles was obtained, which enhanced the effective specific surface area and electrochemical activity of the working electrode. Therefore, wide detection concentration ranges for Hg(II) of 5 to 1000 µg/L and for As(III) of 5 to 5000 µg/L were displayed, with detection limits of 1.4 µg/L and 2.4 µg/L, respectively. Moreover, the sensor exhibited satisfactory reproducibility, stability and anti-interference capability. These characteristics enable the developed microelectrode sensor chip to be utilized in the monitoring of a diverse range of pollution sources. Full article

Here, we present the results of our the electrochemical aptasensing strategy for retinol binding protein-4 (RBP-4) detection based on a thiolated aptamer against RBP-4 and 6-mercaptohexanol (MCH) directly immobilized on a gold electrode surface. The most important parameters affecting the magnitude of the analytical signal generated were optimized: (i) the presence of magnesium ions in the immobilization and measurement buffer, (ii) the concentration of aptamer in the immobilization solution and (iii) its folding procedure. In this work, a systematic assessment of the electrochemical parameters related to the optimization of the sensing layer of the aptasensor was carried out (electron transfer coefficients (α), electron transfer rate constants (k⁰) and surface coverage of the thiolated aptamer probe (Γ_Apt)). Then, under the optimized conditions, the analytical response towards RBP-4 protein, in the presence of an Fe(CN)₆^3−/4− redox couple in the supporting solution was assessed. The proposed electrochemical strategy allowed for RBP-4 detection in the concentration range between 100 and 1000 ng/mL with a limit of detection equal to 44 ng/mL based on electrochemical impedance spectroscopy (EIS). The specificity studies against other diabetes biomarkers, including vaspin and adiponectin, proved the selectivity of the proposed platform. These preliminary results will be used in the next step to miniaturize and test the sensor in real samples. Full article

A surface-enhanced Raman scattering (SERS) method for measuring nitrate nitrogen in aquaculture water was developed using a substrate of β-cyclodextrin-modified gold nanoparticles (SH-β-CD@AuNPs). Addressing the issues of low sensitivity, narrow linear range, and relatively poor selectivity of single metal nanoparticles in the SERS detection of nitrate nitrogen, we combined metal nanoparticles with cyclodextrin supramolecular compounds to prepare a AuNPs substrate enveloped by cyclodextrin, which exhibits ultra-high selectivity and Raman activity. Subsequently, vanadium(III) chloride was used to convert nitrate ions into nitrite ions. The adsorption mechanism between the reaction product benzotriazole (BTAH) of o-phenylenediamine (OPD) and nitrite ions on the SH-β-CD@AuNPs substrate was studied through SERS, achieving the simultaneous detection of nitrate nitrogen and nitrite nitrogen. The experimental results show that BTAH exhibits distinct SERS characteristic peaks at 1168, 1240, 1375, and 1600 cm⁻¹, with the lowest detection limits of 3.33 × 10⁻², 5.84 × 10⁻², 2.40 × 10⁻², and 1.05 × 10⁻² μmol/L, respectively, and a linear range of 0.1–30.0 μmol/L. The proposed method provides an effective tool for the selective and accurate online detection of nitrite and nitrate nitrogen in aquaculture water. Full article

Novel dihydroquinoline derivatives (DHP and DHP-OH) were synthesized in one pot via a tandem trimerization-cyclization of methylpropiolate. DHP and DHP-OH possess strong blue fluorescence with high quantum efficiencies over 0.70 in aqueous media. DHP-OH displays a remarkable fluorescence quenching selectively to the presence of Au³⁺ through the oxidation of dihydropyridine to pyridinium ion as confirmed by NMR and HRMS. DHP-OH was used to demonstrate the quantitative analysis of Au³⁺ in water samples with the limit of detection of 33 ppb and excellent recovery (>95%). This fluorescent probe was also applied for the determination of Au³⁺ residue in the gold nanoparticle solution and a paper-based sensing strip for the on-site detection of Au³⁺. Full article

Novel Cr(III)-imprinted poly(vinyl alcohol)/sodium alginate/AuNPs hydrogel membranes (Cr(III)-IIMs) were obtained and characterized and further applied as a sorbent for chromium speciation in waters. Cr(III)-IIMs were prepared via solution blending method using blends of poly(vinyl alcohol) and sodium alginate as film-forming materials, poly(ethylene glycol) as a porogen agent, sodium alginate stabilized gold nanoparticles (SA-AuNPs) as a crosslinking and mechanically stabilizing component, and Cr(III) ions as a template species. The physicochemical characteristics of pre-synthesized AuNPs and obtained hydrogel membranes Cr(III)-IIM were studied by UV-vis and FTIR spectroscopy, TEM and SEM observations, N₂ adsorption–desorption measurements, and XRD analysis. The mechanism of the adsorption process toward Cr(III) was best described by pseudo-first-order kinetic and Langmuir models. Experiments performed showed that quantitative retention of Cr(III) is attained in 20 h at pH 6 and temperature 40 °C. Under the same conditions, the adsorption of Cr(VI) is below 5%. A simple and sensitive analytical procedure was developed for the speciation of Cr in an aquatic environment using dispersive solid phase extraction of Cr(III) by Cr(III)-IIM prior to selective Cr(VI) measurement by ETAAS in the supernatants. The detection limits and reproducibility achieved for the Cr speciation analysis fulfill the requirements for their monitoring in waters under the demand of the Water Framework Directive. Full article

Environmental pollution with cadmium (Cd) is a major concern worldwide, with prolonged exposure to this toxic heavy metal causing serious health problems, such as kidney damage, cancer, or cardiovascular diseases, only to mention a few. Herein, a gold-coated reflection-type fiber optic–-surface plasmon resonance (Au-coated FO-SPR) sensor is manufactured and functionalized with (i) bovine serum albumin (BSA), (ii) chitosan, and (iii) polyaniline (PANI), respectively, for the sensitive detection of cadmium ions (Cd${}^{2+}$) in water. Then, the three sensor functionalization strategies are evaluated and compared one at a time. Out of these strategies, the BSA-functionalized FO-SPR sensor is found to be highly sensitive, exhibiting a limit of detection (LOD) for Cd${}^{2+}$ detection at nM level. Moreover, the presence of Cd${}^{2+}$ on the FO-SPR sensor surface was confirmed by the X-ray photoelectron spectroscopy (XPS) technique and also quantified consecutively for all the above-mentioned functionalization strategies. Hence, the BSA-functionalized FO-SPR sensor is sensitive, provides a rapid detection time, and is cheap and portable, with potential applicability for monitoring trace-level amounts of Cd within environmental or potable water. Full article

The development of reliable and highly sensitive methods for heavy metal detection is a critical task for protecting the environment and human health. In this study, a qualitative colorimetric sensor that used mercaptosuccinic-acid-functionalized gold nanoparticles (MSA-AuNPs) to detect trace amounts of Fe(III) ions was developed. MSA-AuNPs were prepared using a one-step reaction, where mercaptosuccinic acid (MSA) was used for both stabilization, which was provided by the presence of two carboxyl groups, and functionalization of the gold nanoparticle (AuNP) surface. The chelating properties of MSA in the presence of Fe(III) ions and the concentration-dependent aggregation of AuNPs showed the effectiveness of MSA-AuNPs as a sensing probe with the use of an absorbance ratio of A₅₃₀/A₆₅₀ as an analytical signal in the developed qualitative assay. Furthermore, the obvious Fe(III)-dependent change in the color of the MSA-AuNP solution from red to gray-blue made it possible to visually assess the metal content in a concentration above the detection limit with an assay time of less than 1 min. The detection limit that was achieved (23 ng/mL) using the proposed colorimetric sensor is more than 10 times lower than the maximum allowable concentration for drinking water defined by the World Health Organization (WHO). The MSA-AuNPs were successfully applied for Fe(III) determination in tap, spring, and drinking water, with a recovery range from 89.6 to 126%. Thus, the practicality of the MSA-AuNP-based sensor and its potential for detecting Fe(III) in real water samples were confirmed by the rapidity of testing and its high sensitivity and selectivity in the presence of competing metal ions. Full article

Solid-contact ion-selective electrodes for histamine (HA) determination were fabricated and studied. Gold wire (0.5 mm diameter) was coated with poly(3,4-ethlenedioxythiophene) doped with poly(styrenesulfonate) (PEDOT:PSS) as a solid conductive layer. The polyvinyl chloride matrix embedded with 5,10,15,20-tetraphenyl(porphyrinato)iron(iii) chloride as an ionophore, 2-nitrophenyloctyl ether as a plasticizer and potassium tetrakis(p-chlorophenyl) borate as an ion exchanger was used to cover the PEDOT:PSS layer as a selective membrane. The characteristics of the HA electrodes were also investigated. The detection limit of 8.58 × 10⁻⁶ M, the fast response time of less than 5 s, the good reproducibility, the long-term stability and the selectivity in the presence of common interferences in biological fluids were satisfactory. The electrode also performed stably in the pH range of 7–8 and the temperature range of 35–41 °C. Additionally, the recovery rate of 99.7% in artificial cerebrospinal fluid showed the potential for the electrode to be used in biological applications. Full article

The application of mercaptosuccinic acid-capped gold nanoparticles as a sensing probe for the colorimetric detection of Fe(III) is reported. The well-dispersed gold nanoparticles (AuNPs) with a diameter of around 20 nm were obtained by a one-step reaction of tetrachloroauratic acid with mercaptosuccinic acid (MSA) as a reducing and capping agent, respectively. Fe(III) reportedly causes the aggregation of prepared MSA-capped AuNPs followed by a change in color and a shift to long wavelengths in the absorbance spectra. The resulting method allows for a visual and spectrophotometric Fe(III) determination with detection limits of 30 ng/mL and 23 ng/mL, respectively. MSA-capped AuNPs have been used as sensing probes for the detection of Fe(III) in drinking water samples with a detection limit that is much lower than the maximum permissible level of Fe(III) specified by official regulations (300 ng/mL). Full article

The widespread presence of heavy metals in drinking water sources arises as a major health concern, particularly in developing countries. The development of low-cost and reliable detection techniques is identified as a societal need to provide affordable water quality control. Herein, a bismuth film-coated gold ultramicroelectrode array (BF-UMEA) was used for the detection of Pb(II) and Cd(II) in water samples via square wave anodic stripping voltammetry (SWASV). Experimental parameters such as deposition time, Bi(III) concentration, acetate buffer concentration, pH, square wave frequency, amplitude, and step potential were all varied to determine their effects on the current peak intensities of the target metal ions. Ten-fold excess in the concentration of interferences was found to cause a decrease in the stripping peak areas of Cd(II) and Pb(II) in the following order of magnitude: benzene < NaCl < Ni(II) < Cu(II). Using Box–Behnken design, the optimum SWASV parameters that provided maximum current peak areas were 14.76 Hz (frequency), 50.10 mV (amplitude), and 8.76 mV (step potential). The limits of detection of the as-prepared BF-UMEA were 5 and 7 µg L⁻¹ for Pb(II) and Cd(II), respectively. These results demonstrate the potential use of a BF-UMEA in SWASV for the trace quantification of Pb(II) and Cd(II) in water samples. Full article

We report the generation of gold nanoparticles (AuNPs) from the aqueous solution of chloro(2,2′,2″-terpyridine)gold(III) ion ([Au(tpy)Cl]²⁺) through X-ray radiolysis and optical excitation at a synchrotron. The original purpose of the experiment was to investigate the photoinduced structural changes of [Au(tpy)Cl]²⁺ upon 400 nm excitation using time-resolved X-ray liquidography (TRXL). Initially, the TRXL data did not show any signal that would suggest structural changes of the solute molecule, but after an induction time, the TRXL data started to show sharp peaks and valleys. In the early phase, AuNPs with two types of morphology, dendrites, and spheres, were formed by the reducing action of hydrated electrons generated by the X-ray radiolysis of water, thereby allowing the detection of TRXL data due to the laser-induced lattice expansion and relaxation of AuNPs. Along with the lattice expansion, the dendritic and spherical AuNPs were transformed into smaller, raspberry-shaped AuNPs of a relatively uniform size via ablation by the optical femtosecond laser pulse used for the TRXL experiment. Density functional theory calculations confirm that the reduction potential of the metal complex relative to the hydration potential of X-ray-generated electrons determines the facile AuNP formation observed for [Au(tpy)Cl]²⁺. Full article

A simple and rapid positive–negative colorimetric approach to determine the presence of antimony ions based on the use of gold nanoparticles conjugated with oligonucleotide (poly-A sequence) is developed. Colorimetric measurements reveal that the aggregates of modified gold nanoparticles were afforded after adding antimony ions, thus changing the solution color from pink to blue. The results of aptamer’s interaction on the gold nanoparticle surface with the target analyte can be detected either by photometry or by the naked eye. The realized assay provides rapid (2 min), sensitive (detection limit 10 ng/mL), specific, and precise (variation coefficient less than 3.8%) detection of antimony (III) in drinking water. Full article

This work presents a simple green synthesis of gold nanoparticles (AuNPs) by using an aqueous extract of Etlingera elatior (torch ginger). The metabolites present in E. elatior, including sugars, proteins, polyphenols, and flavonoids, were known to play important roles in reducing metal ions and supporting the subsequent stability of nanoparticles. The present work aimed to investigate the ability of the E. elatior extract to synthesise AuNPs via the reduction of gold (III) chloride hydrate and characterise the properties of the nanoparticles produced. The antioxidant properties of the E. elatior extract were evaluated by analysing the total phenolic and total flavonoid contents. To ascertain the formation of AuNPs, the synthesised particles were characterised using the ultraviolet-visible (UV-Vis) spectroscopy, Fourier transform infrared (FTIR) spectroscopy, high-resolution transmission electron microscopy (HRTEM), energy-dispersive X-ray (EDX) microscopy, and dynamic light scattering (DLS) measurement. The properties of the green synthesised AuNPs were shown to be comparable to the AuNPs produced using a conventional reducing agent, sodium citrate. The UV-Vis measured the surface plasmon resonance of the AuNPs, and a band centered at 529 nm was obtained. The FTIR results proved that the extract contained the O-H functional group that is responsible for capping the nanoparticles. The HRTEM images showed that the green synthesized AuNPs were of various shapes and the average of the nanoparticles’ hydrodynamic diameter was 31.5 ± 0.5 nm. Meanwhile, the zeta potential of −32.0 ± 0.4 mV indicates the high stability and negative charge of the AuNPs. We further successfully demonstrated that using the green synthesised AuNPs as the nanocomposite to modify the working surface of screen-printed carbon electrode (SPCE/Cs/AuNPs) enhanced the rate of electron transfer and provided a sensitive platform for the detection of Cu(II) ions. Full article

Techniques of stripping voltammetry (SV) determination of silver and gold in pyrites and carbonaceous matter are developed. The problem of quantitative transfer of the analytes into the solution is solved. For this purpose, the ore matrix of carbonaceous shales was decomposed by mineral acids in autoclaves at high pressures. The element to be determined from the sample matrix was separated by extraction. Ag(I) ions from the solutions were extracted in the form of a dithizonate complex in CCl₄. Au(III) ions were extracted by diethyl ether. The extracts were decomposed thermally. The dry residue was dissolved in the background electrolyte, and the element was determined by the SV method. The graphite electrode (GE) impregnated with polyethylene was used as a working electrode in the SV determination of silver. The SV determination of gold was carried out using a GE modified by bismuth. The limits of detection (LOD) of Ag(I) and Au(III) contents were equal to 0.016 mg L⁻¹ and 0.0086 mg L⁻¹, respectively. The results of SV determination of gold and silver in standard samples, pyrites, and carbonaceous shales were presented. The silver content in the pyrite was 13.6 g t⁻¹, and in carbon shale it was 0.34 g t⁻¹. The concentration of gold in the pyrite of the Kirovsko–Kryklinskaya ore zone was 1.15 g t⁻¹, while in carbonaceous shales it was 2.66 g t⁻¹. The obtained data were consistent with the data of atomic emission spectroscopy (AES) and inductively-coupled plasma mass spectrometry (ICP–MS). The error of determination of elements by stripping voltammetry was calculated as ranging from 10 to 6 g t⁻¹ (less than 12%) in pyrite and carbonaceous material when determining the silver content, and from 1 to 3 g t⁻¹ (less than 22%) when determining the gold content in pyrite and carbonaceous matter. Full article